CN113939736A - Liquefied carbon dioxide supply device and supercritical fluid device - Google Patents

Liquefied carbon dioxide supply device and supercritical fluid device Download PDF

Info

Publication number
CN113939736A
CN113939736A CN201980097252.1A CN201980097252A CN113939736A CN 113939736 A CN113939736 A CN 113939736A CN 201980097252 A CN201980097252 A CN 201980097252A CN 113939736 A CN113939736 A CN 113939736A
Authority
CN
China
Prior art keywords
flow path
carbon dioxide
liquefied carbon
supply device
dioxide supply
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201980097252.1A
Other languages
Chinese (zh)
Other versions
CN113939736B (en
Inventor
高良智寻
佐藤刚志
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Publication of CN113939736A publication Critical patent/CN113939736A/en
Application granted granted Critical
Publication of CN113939736B publication Critical patent/CN113939736B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/30Control of physical parameters of the fluid carrier of temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/26Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/40Selective adsorption, e.g. chromatography characterised by the separation mechanism using supercritical fluid as mobile phase or eluent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/16Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
    • B01D15/161Temperature conditioning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/30Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3092Heat exchange between incoming and outgoing mobile phase

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The liquefied carbon dioxide supply device is configured to supply liquefied carbon dioxide to a supercritical fluid device including a separation column, and includes a first channel section, a second channel section, a compressor, a heat exchanger, and a pump section. The compressor circulates a first refrigerant through the first flow path portion to repeat a refrigeration cycle. The heat exchanger exchanges heat between the first channel portion and the second channel portion. The pump section supplies the liquefied carbon dioxide flowing through the second flow path section to the separation column of the supercritical fluid device.

Description

Liquefied carbon dioxide supply device and supercritical fluid device
Technical Field
The present invention relates to a liquid feeding and supplying apparatus for liquefied carbon dioxide and a supercritical fluid apparatus.
Background
In a Supercritical Fluid apparatus such as a Supercritical Fluid Chromatograph (SFC) or a Supercritical Fluid extraction apparatus (Supercritical Fluid Extractor (SFE)), a sample is analyzed or collected using a Supercritical Fluid as a mobile phase. For example, in the SFC described in patent document 1, liquefied carbon dioxide is supplied as a mobile phase to a mobile phase flow path by a liquid-feeding pump. Further, the sample is injected into the mobile phase channel by the sample injection section.
The mobile phase and the sample pass through a separation column disposed in the mobile phase flow path. Here, the pressure in the mobile phase flow path is maintained by a back pressure valve and the temperature of the separation column is maintained by a column oven so that the mobile phase becomes at least in a supercritical state in the separation column. The sample is separated for each sample component by passing through the separation column, and is detected by a detector.
Patent document 1: japanese patent laid-open publication No. 2016-173343
Disclosure of Invention
[ problems to be solved by the invention ]
In a supercritical fluid extraction apparatus, a flow path of carbon dioxide is cooled in order to maintain carbon dioxide in a liquid phase. When the capacity of liquefied carbon dioxide is large, a cooler (chiller) is generally used for cooling the flow path. However, the cooler is relatively large and is mostly installed on the floor. Therefore, the installation space for the cooler becomes large, and the supercritical fluid apparatus becomes large. Further, since the piping is indirectly cooled using a refrigerant such as water, the temperature of the liquefied carbon dioxide cannot be stably controlled. In this case, as the density of the liquefied carbon dioxide becomes unstable, the flow rate of the liquefied carbon dioxide becomes unstable.
The purpose of the present invention is to provide a liquefied carbon dioxide liquid-feeding supply device and a supercritical fluid device capable of supplying liquefied carbon dioxide at a stable flow rate while suppressing an increase in size.
[ means for solving problems ]
An aspect according to an aspect of the present invention relates to a liquefied carbon dioxide supply apparatus that supplies liquefied carbon dioxide to a supercritical fluid apparatus including a separation column, the liquefied carbon dioxide supply apparatus including: a first channel section and a second channel section; a compressor that circulates a first refrigerant through the first channel portion to repeat a refrigeration cycle; a heat exchanger that exchanges heat between the first channel portion and the second channel portion; and a pump section for supplying the liquefied carbon dioxide flowing through the second channel section to the separation column.
[ Effect of the invention ]
According to the present invention, liquefied carbon dioxide can be supplied at a stable flow rate while suppressing an increase in size of the liquefied carbon dioxide liquid supply and supply device and the supercritical fluid device.
Drawings
Fig. 1 is a diagram showing a structure of a supercritical fluid apparatus according to an embodiment of the present invention.
Fig. 2 is a diagram showing a configuration of the liquefied carbon dioxide supply device of fig. 1.
Detailed Description
(1) Structure of supercritical fluid device
Hereinafter, a liquefied carbon dioxide liquid feeding and supplying apparatus and a supercritical fluid apparatus according to an embodiment of the present invention will be described in detail with reference to the drawings. Fig. 1 is a diagram showing a structure of a supercritical fluid apparatus according to an embodiment of the present invention. As shown in fig. 1, the supercritical fluid apparatus 200 is a Supercritical Fluid Chromatograph (SFC) including: a liquefied carbon dioxide supply device 100, a modifier (modifier) supply device 110, a mixing unit 120, a sample supply unit 130, a separation column 140, a detector 150, a back pressure valve 160, and a control unit 170.
Supercritical fluid apparatus 200 is provided with bottle 201 and bottle 202. In bottle 201, liquefied carbon dioxide, for example cooled to about 5 ℃, is stored as a mobile phase. The liquefied carbon dioxide supply device 100 cools and pressure-feeds the liquefied carbon dioxide stored in the bottle 201. The details of the liquefied carbon dioxide supply apparatus 100 will be described later.
In the bottle 202, a modifier such as an organic solvent is stored as a mobile phase. Modifier supply device 110 is, for example, a liquid feeding pump, and pumps modifier stored in bottle 202 under pressure. The mixing section 120 is, for example, a gradient mixer (gradient mixer) and supplies the mobile phases pumped and supplied from the liquefied carbon dioxide supply apparatus 100 and the modifier supply apparatus 110 at a predetermined ratio while mixing them.
The sample supply unit 130 is, for example, an ejector (injector), and introduces a sample to be analyzed and the mobile phase supplied from the mixing unit 120 into the separation column 140. The separation column 140 is housed in a column thermostat, not shown, and is heated to a predetermined temperature (about 40 ℃ in the present example) so that the liquefied carbon dioxide in the introduced mobile phase is in a supercritical state. The separation column 140 separates the introduced sample into components according to the difference in chemical properties or composition.
The detector 150 is, for example, an absorbance detector, and detects components of the sample separated by the separation column 140. The detection result obtained by the detector 150 is used to generate, for example, a supercritical fluid chromatogram showing the relationship between the retention time and the detection intensity of each component. The back pressure valve 160 maintains the pressure in the flow path of the mobile phase at a pressure equal to or higher than the critical pressure of carbon dioxide (for example, 8MPa) so that the liquefied carbon dioxide in the mobile phase is in a supercritical state at least in the separation column 140.
The control Unit 170 includes a Central Processing Unit (CPU), a memory, a microcomputer, or the like, and controls the operations of the liquefied carbon dioxide supply device 100, the modifier supply device 110, the mixing Unit 120, the sample supply Unit 130, the separation column 140 (column thermostat), the detector 150, and the back pressure valve 160. In the case where a separator such as a fraction collector (fraction collector) is provided downstream of the back pressure valve 160, the control unit 170 further controls the operation of the separator based on the detection result obtained by the detector 150. The control unit 170 may be provided in the back pressure valve 160.
(2) Structure of liquefied carbon dioxide supply device
Fig. 2 is a diagram showing a configuration of the liquefied carbon dioxide supply apparatus 100 shown in fig. 1. As shown in fig. 2, the liquefied carbon dioxide supply device 100 includes a cooling unit 10 and a pump unit 20. The liquefied carbon dioxide supply device 100 is provided with a flow path unit 1, a flow path unit 2, and a flow path unit 3. The flow path portions 1 to 3 are, for example, pipes. The flow path portions 1 to 3 are examples of first to third flow path portions, respectively. In the following description, the flow path section 2 and the flow path section 3 define the direction in which the liquefied carbon dioxide or the refrigerant flows as the downstream direction, and the opposite direction as the upstream direction.
The cooling portion 10 includes: heat exchanger 11, compressor 12, reservoir 13, and liquid feed 14. The heat exchanger 11 includes a block portion 11a and a metal material 11 b. The block 11a includes four side surfaces, an upper surface, and a bottom surface formed of a metal plate, and has a rectangular parallelepiped shape. The block 11a accommodates a part of each of the flow path section 1, the flow path section 2, and the flow path section 3. The metal material 11b contains, for example, tin, and is filled into the block portion 11a in a molten state. Thus, in the block 11a, gaps among the flow path section 1, the flow path section 2, and the flow path section 3 are filled with the metal material 11 b.
Both ends of the flow path portion 1 are drawn out from the block portion 11a and connected to the compressor 12. The compressor 12 circulates a refrigerant such as fluorocarbon 407C (R-407C) through the flow path portion 1 to repeat the refrigeration cycle. Thereby, the inside of the block portion 11a is cooled. In this example, the flow path section 1 is provided in the block section 11a in a state of being wound in a coil shape. Therefore, even when the sufficiently long flow path section 1 is used, the block section 11a is maintained compact. Therefore, by using the sufficiently long flow path section 1, the inside of the block section 11a can be sufficiently cooled.
The flow path section 2 connects the bottle 201 and the mixing section 120. The heat exchanger 11 and the pump unit 20 are inserted into the flow path portion 2 from upstream to downstream. In the block portion 11a, heat is exchanged between the flow path portion 1 and the flow path portion 2 via the metal material 11 b. Thereby, the liquefied carbon dioxide supplied from bottle 201 to mixing unit 120 is cooled. In this example, the flow path section 2 is provided so as to meander within the block section 11 a. Therefore, the portion of the flow path section 2 provided in the block section 11a can be made long. Therefore, the liquefied carbon dioxide can be sufficiently cooled.
The storage unit 13 is, for example, a bottle, and stores a refrigerant such as ethylene glycol having a concentration of 60%. The liquid feeding unit 14 is, for example, a diaphragm pump (diaphragm pump), and pumps the refrigerant stored in the storage unit 13 to the pump unit 20 through the channel unit 3. The heat exchanger 11 is inserted into a portion of the channel section 3 between the liquid feeding section 14 and the pump section 20. In the block portion 11a, heat is exchanged between the flow path portion 1 and the flow path portion 3 via the metal material 11 b. Thereby, the refrigerant supplied from the liquid feeding portion 14 to the pump portion 20 is cooled. The refrigerant supplied to the pump unit 20 passes through the channel unit 3 and returns to the reservoir unit 13.
In this example, the pump section 20 is a parallel plunger pump, and includes two pump heads 21 and 22. In the pump section 20, the channel section 2 includes a main channel section 2a, a main channel section 2b, a branch channel section 2c, and a branch channel section 2 d. The main channel portion 2a and the main channel portion 2b are connected to the cooling portion 10 and the mixing portion 120, respectively. The branch channel part 2c and the branch channel part 2d are disposed in parallel so as to branch into two channels between the main channel part 2a and the main channel part 2 b. The pump head 21 and the pump head 22 are inserted into the branch flow path part 2c and the branch flow path part 2d, respectively, and the liquefied carbon dioxide stored in the bottle 201 is alternately pressure-fed to the mixing part 120 through the cooling part 10.
In the pump section 20, the channel section 3 includes a main channel section 3a, a main channel section 3b, a branch channel section 3c, and a branch channel section 3 d. The main flow path portion 3a and the main flow path portion 3b are connected to the heat exchanger 11 and the reservoir portion 13 of the cooling unit 10, respectively. The branch flow path section 3c and the branch flow path section 3d are disposed in parallel so as to branch into two flow paths between the main flow path section 3a and the main flow path section 3b, and are attached to the surfaces of the pump heads 21 and 22, respectively. The refrigerant supplied from the heat exchanger 11 through the main channel portion 3a flows through the branch channel portion 3c and the branch channel portion 3 d. Thereby, the pump heads 21 and 22 are cooled. The refrigerant flowing through the branch flow path portion 3c and the branch flow path portion 3d passes through the main flow path portion 3b and returns to the reservoir portion 13.
(3) Operation of the control section
According to the cooling mechanism, in the heat exchanger 11, the flow path section 1 is cooled to, for example, about-30 ℃, and the flow path sections 2 and 3 are cooled to, for example, about-10 ℃. On the other hand, the temperature of the liquefied carbon dioxide flowing through the passage portion 2 is preferably other values (about 5 ℃ in the present example). The temperatures of the pump heads 21 and 22 are preferably other values (about 5 ℃ in this example).
Therefore, the heating unit 15 and the heating unit 16 are attached to the downstream portions of the flow path section 2 and the flow path section 3, respectively, which are drawn out from the block 11 a. The heating unit 15 and the heating unit 16 are examples of a first heating unit and a second heating unit, respectively. Further, a temperature sensor 4 is mounted on the surface of the flow path portion 2 downstream of the heating portion 15. Further, a temperature sensor 5 and a temperature sensor 6 are attached to the surfaces of the pump heads 21 and 22, respectively. The temperature sensors 4 to 6 each include, for example, a thermistor (thermistor). The temperature sensor 4 is an example of a first temperature sensor, and the temperature sensors 5 and 6 are examples of a second temperature sensor. The operations of the heating portions 15 and 16 are independently controlled by the control portion 170 of fig. 1.
Specifically, the operation of the heating portion 15 is controlled so that the temperature detected by the temperature sensor 4 becomes a desired temperature. Here, since the temperature sensor 4 is directly attached to the surface of the flow path unit 2, the temperature of the liquefied carbon dioxide flowing through the flow path unit 2 is accurately detected as the temperature of the flow path unit 2. Therefore, the temperature of the liquefied carbon dioxide flowing through the flow path portion 2 can be maintained at a desired temperature by the control. The temperature sensor 4 can be fixed to the flow path portion 2 by an electrically conductive adhesive tape or an electrically conductive adhesive having high thermal conductivity. In this case, the temperature of the flow path section 2 can be detected with higher accuracy.
Similarly, the operation of the heating unit 16 is controlled so that the temperatures detected by the temperature sensors 5 and 6 become desired temperatures. This can maintain the temperature of the pump heads 21 and 22 at a desired temperature. The temperature sensors 5 and 6 may be directly attached to the surfaces of the branch flow path section 3c and the branch flow path section 3d, and the temperatures of the pump head 21 and the pump head 22 may be detected as the temperatures of the branch flow path section 3c and the branch flow path section 3d, respectively.
(4) Effect
In the supercritical fluid apparatus 200 according to the present embodiment, since it is not necessary to use a cooler for cooling the flow path section 2, the size increase of the liquefied carbon dioxide supply apparatus 100 is suppressed. In this case, the liquefied carbon dioxide supply device 100 may be mounted on a table, rather than on a floor. Therefore, a wide space can be secured in the supercritical fluid apparatus 200, and space can be saved.
Further, the flow path portion 2 can be directly cooled without using a refrigerant such as water. Therefore, the temperature of the liquefied carbon dioxide becomes stable, and thereby the density of the liquefied carbon dioxide becomes stable. As a result, liquefied carbon dioxide can be supplied at a stable flow rate while suppressing an increase in size of the liquefied carbon dioxide supply apparatus 100 and the supercritical fluid apparatus 200.
The flow path section 2 is heated by the heating section 15 based on the temperature detected by the temperature sensor 4. Here, since the temperature sensor 4 is directly attached to the surface of the flow path unit 2, the temperature of the flow path unit 2 can be accurately detected as the temperature of the liquefied carbon dioxide flowing through the flow path unit 2. Therefore, the temperature of the liquefied carbon dioxide can be easily adjusted to a desired temperature. This makes it possible to supply liquefied carbon dioxide at a more stable flow rate.
When the flow rate of the liquefied carbon dioxide is small, the temperature of the liquefied carbon dioxide is likely to fluctuate in the portion of the flow path section 2 from the heat exchanger 11 to the pump section 20 due to the influence of the outside air. In this case, heat is also exchanged between the flow path section 1 and the flow path section 3 by the heat exchanger 11. Further, based on the temperatures of the pump head 21 and the pump head 22 detected by the temperature sensor 5 and the temperature sensor 6, respectively, the temperature of the flow path section 3 is adjusted by the heating section 16 so as to be a desired temperature. Thereby, the pump heads 21 and 22 are cooled to a desired temperature via the refrigerant flowing through the flow path section 3. As a result, the temperature of the liquefied carbon dioxide supplied from the pump section 20 can be further stabilized.
(5) Other embodiments
(a) In the above embodiment, the cooling unit 10 is configured to be able to cool the pump head 21 and the pump head 22 of the pump unit 20, but the embodiment is not limited thereto. The cooling unit 10 may not be configured to be able to cool the pump head 21 and the pump head 22 of the pump unit 20 when the temperatures of the pump head 21 and the pump head 22 are sufficiently stable or when the temperatures of the pump head 21 and the pump head 22 are adjusted by another temperature adjustment device.
(b) In the above embodiment, the heating portion 15 is attached to the downstream portion of the flow path portion 2 drawn out from the block portion 11a, but the embodiment is not limited thereto. The heating section 15 may be installed in an upstream portion of the flow path section 2 drawn from the block section 11 a. In this case, the temperature sensor 4 is also attached to the flow path section 2 further downstream than the heat exchanger 11 and the heating section 15.
Similarly, the heating unit 16 is attached to a downstream portion of the flow path unit 3 drawn out from the block 11a, but the embodiment is not limited thereto. The heating section 16 may be installed in an upstream portion of the flow path section 3 drawn from the block section 11 a.
When the liquefied carbon dioxide flowing through the flow path section 2 is cooled to a desired temperature by the heat exchanger 11, the heating section 15 may not be attached to the flow path section 2. When the pump head 21 and the pump head 22 are cooled to a desired temperature by the heat exchanger 11, the heating unit 16 may not be attached to the flow path section 3.
(c) In the above embodiment, the supercritical fluid apparatus 200 is configured as SFC, but the embodiment is not limited thereto. Supercritical fluid apparatus 200 may also be configured as a supercritical fluid extraction apparatus (SFE). Alternatively, the supercritical fluid apparatus 200 may be configured to include a Mass Spectrometer (MS) instead of the SFC-MS of the detector 150.
(6) Form of the composition
The liquefied carbon dioxide supply device according to the (item 1) above
Supplying liquefied carbon dioxide to a supercritical fluid apparatus including a separation column, the liquefied carbon dioxide supply apparatus including:
a first channel section and a second channel section;
a compressor that circulates a first refrigerant through the first channel portion to repeat a refrigeration cycle;
a heat exchanger that exchanges heat between the first channel portion and the second channel portion; and
and a pump section for supplying the liquefied carbon dioxide flowing through the second channel section to the separation column.
In the liquefied carbon dioxide supply device, the first refrigerant is circulated through the first flow path unit by the compressor so that the refrigeration cycle is repeated. In this case, in the heat exchanger, heat is exchanged between the first channel portion and the second channel portion, and the second channel portion is cooled. Therefore, the liquefied carbon dioxide flowing through the second flow path portion is cooled. The liquefied carbon dioxide cooled in the second channel section is supplied to the separation column of the supercritical fluid device by the pump section.
According to the above configuration, since it is not necessary to use a cooler for cooling the second flow path portion, the size of the liquefied carbon dioxide supply device can be suppressed from increasing. Further, the second channel portion can be directly cooled without using a refrigerant such as water. Therefore, the temperature of the liquefied carbon dioxide becomes stable, and thereby the density of the liquefied carbon dioxide becomes stable. As a result, the liquefied carbon dioxide can be supplied at a stable flow rate while suppressing an increase in the size of the liquefied carbon dioxide supply device.
(item 2) the liquefied carbon dioxide supply apparatus according to item 1, may be
The heat exchanger includes:
a block portion having an internal space for accommodating a part of the first channel portion and a part of the second channel portion; and
and a metal material filled in the internal space of the block portion so as to fill a gap between the first channel portion and the second channel portion.
In this case, heat can be efficiently exchanged between the first channel portion and the second channel portion via the metal material.
(item 3) the liquefied carbon dioxide supply apparatus according to item 1 or 2, wherein
Further, the apparatus includes a first heating unit that heats the second channel unit.
In this case, the temperature of the second channel portion can be easily maintained at a desired temperature by heating the second channel portion. This allows the liquefied carbon dioxide flowing through the second flow path portion to be maintained at a desired temperature.
(item 4) the liquefied carbon dioxide supply apparatus according to item 3, may be
The heat exchanger further includes a first temperature sensor that is attached to the second flow path portion and detects a temperature of the second flow path portion, downstream of the heat exchanger and the first heating unit.
In this case, since the first temperature sensor is attached to the second channel portion, the temperature of the second channel portion can be accurately detected as the temperature of the liquefied carbon dioxide flowing through the second channel portion. Therefore, the temperature of the liquefied carbon dioxide flowing through the second flow path portion can be easily adjusted by the first heating unit based on the detected temperature. This makes it possible to supply liquefied carbon dioxide at a more stable flow rate.
(item 5) the liquefied carbon dioxide supply apparatus according to item 1 or 2, wherein
Further comprises a third flow path part for circulating the second refrigerant,
the heat exchanger further exchanges heat between the first flow path portion and the third flow path portion,
the pump section includes a pump head to which a part of the third channel section is attached.
When the flow rate of the liquefied carbon dioxide is small, the temperature of the liquefied carbon dioxide is likely to vary in the portion from the heat exchanger to the second channel portion of the pump portion due to the influence of the outside air. In this case, according to the above configuration, the pump head is also cooled by the third flow path portion. This makes it possible to further stabilize the temperature of the liquefied carbon dioxide supplied from the pump unit.
(item 6) the liquefied carbon dioxide supply apparatus according to item 5, wherein
Further, the apparatus includes a second heating unit that heats the third channel unit.
In this case, the temperature of the third channel part can be easily maintained at a desired temperature by heating the third channel part. Thus, the temperature of the pump head can be maintained at a desired temperature via the second refrigerant flowing through the third flow path portion. As a result, the temperature of the liquefied carbon dioxide supplied from the pump section can be maintained at a desired temperature.
(item 7) the liquefied carbon dioxide supply apparatus according to item 6, wherein
Further comprising a second temperature sensor for detecting the temperature of the pump head.
In this case, the temperature of the third flow path section can be easily adjusted by the second heating unit based on the temperature detected by the second temperature sensor.
The supercritical fluid apparatus according to another aspect (item 8) may include:
a separation column;
the liquefied carbon dioxide supply device according to claim 4, wherein the separation column is supplied with liquefied carbon dioxide; and
and a control unit that controls an operation of the first heating unit such that a temperature detected by the first temperature sensor of the liquefied carbon dioxide supply device becomes a preset temperature.
In the supercritical fluid apparatus, the operation of the first heating unit is controlled by the control unit so that the temperature detected by the first temperature sensor of the liquefied carbon dioxide supply device becomes a preset temperature. Thereby, the temperature of the liquefied carbon dioxide flowing through the second flow path portion is maintained at a desired temperature. According to this configuration, the liquefied carbon dioxide can be supplied to the separation column at a more stable flow rate while suppressing an increase in size of the liquefied carbon dioxide supply device.

Claims (8)

1.一种液化二氧化碳供给装置,对包括分离柱的超临界流体装置供给液化二氧化碳,所述液化二氧化碳供给装置包括:1. A liquefied carbon dioxide supply device, supplying liquefied carbon dioxide to a supercritical fluid device comprising a separation column, the liquefied carbon dioxide supply device comprising: 第一流路部及第二流路部;a first flow path portion and a second flow path portion; 压缩机,使第一制冷剂经过所述第一流路部进行循环以使冷冻循环反复进行;a compressor, which circulates the first refrigerant through the first flow path part to repeat the refrigeration cycle; 热交换器,在所述第一流路部与所述第二流路部之间进行热交换;以及a heat exchanger for exchanging heat between the first flow path portion and the second flow path portion; and 泵部,将在所述第二流路部中流动的液化二氧化碳向所述分离柱供给。The pump part supplies the liquefied carbon dioxide flowing in the second flow path part to the separation column. 2.根据权利要求1所述的液化二氧化碳供给装置,其中所述热交换器包括:2. The liquefied carbon dioxide supply device according to claim 1, wherein the heat exchanger comprises: 块部,具有收容所述第一流路部的一部分及所述第二流路部的一部分的内部空间;以及a block portion having an inner space that accommodates a portion of the first flow path portion and a portion of the second flow path portion; and 金属材料,以填埋所述第一流路部与所述第二流路部的间隙的方式被填充到所述块部的所述内部空间。A metal material is filled in the inner space of the block portion so as to fill the gap between the first flow path portion and the second flow path portion. 3.根据权利要求1或2所述的液化二氧化碳供给装置,进而包括对所述第二流路部进行加热的第一加热部。3. The liquefied carbon dioxide supply device according to claim 1 or 2, further comprising a first heating portion that heats the second flow path portion. 4.根据权利要求3所述的液化二氧化碳供给装置,其中在较所述热交换器及所述第一加热部更靠下游,进而包括安装于所述第二流路部且对所述第二流路部的温度进行检测的第一温度传感器。4 . The liquefied carbon dioxide supply device according to claim 3 , further comprising: downstream of the heat exchanger and the first heating part, and further comprising: the liquefied carbon dioxide supply device installed on the second flow path part and facing the second flow path part. 5 . A first temperature sensor that detects the temperature of the flow path portion. 5.根据权利要求1或2所述的液化二氧化碳供给装置,进而包括供第二制冷剂进行循环的第三流路部,5. The liquefied carbon dioxide supply device according to claim 1 or 2, further comprising a third flow path portion through which the second refrigerant circulates, 所述热交换器进而在所述第一流路部与所述第三流路部之间进行热交换,The heat exchanger further performs heat exchange between the first flow path portion and the third flow path portion, 所述泵部包括安装有所述第三流路部的一部分的泵头。The pump portion includes a pump head to which a part of the third flow path portion is mounted. 6.根据权利要求5所述的液化二氧化碳供给装置,进而包括对所述第三流路部进行加热的第二加热部。6 . The liquefied carbon dioxide supply device according to claim 5 , further comprising a second heating portion that heats the third flow path portion. 7 . 7.根据权利要求6所述的液化二氧化碳供给装置,进而包括对所述泵头的温度进行检测的第二温度传感器。7. The liquefied carbon dioxide supply device according to claim 6, further comprising a second temperature sensor that detects the temperature of the pump head. 8.一种超临界流体装置,包括:8. A supercritical fluid device, comprising: 分离柱;separation column; 根据权利要求4所述的液化二氧化碳供给装置,对所述分离柱供给液化二氧化碳;以及The liquefied carbon dioxide supply device according to claim 4, supplying liquefied carbon dioxide to the separation column; and 控制部,以由所述液化二氧化碳供给装置的所述第一温度传感器检测出的温度成为预先设定的温度的方式,控制所述第一加热部的运行。The control unit controls the operation of the first heating unit so that the temperature detected by the first temperature sensor of the liquefied carbon dioxide supply device becomes a preset temperature.
CN201980097252.1A 2019-06-11 2019-06-11 Liquefied carbon dioxide supply device and supercritical fluid device Active CN113939736B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2019/023156 WO2020250317A1 (en) 2019-06-11 2019-06-11 Liquefied carbon dioxide feeding device and supercritical fluid apparatus

Publications (2)

Publication Number Publication Date
CN113939736A true CN113939736A (en) 2022-01-14
CN113939736B CN113939736B (en) 2024-06-25

Family

ID=73782099

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201980097252.1A Active CN113939736B (en) 2019-06-11 2019-06-11 Liquefied carbon dioxide supply device and supercritical fluid device

Country Status (4)

Country Link
US (1) US12044662B2 (en)
JP (1) JP7342946B2 (en)
CN (1) CN113939736B (en)
WO (1) WO2020250317A1 (en)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5465581A (en) * 1993-08-24 1995-11-14 Hewlett-Packard Analytical system having energy efficient pump
US20100040483A1 (en) * 2008-06-24 2010-02-18 Berger Terry A Compressible fluid pumping system
JP2010101875A (en) * 2008-09-29 2010-05-06 Jasco Corp Device and method for injecting sample in supercritical fluid chromatography
JP2012220030A (en) * 2011-04-04 2012-11-12 Toyo Eng Works Ltd Defrosting device of carbon dioxide circulation and cooling system
US20130334117A1 (en) * 2011-03-10 2013-12-19 Waters Technologies Corporation System and method of cooling a pump head used in chromatography
US20140190183A1 (en) * 2010-05-26 2014-07-10 Agilent Technologies, Inc. Efficient chiller for a supercritical fluid chromatography pump
JP2016173343A (en) * 2015-03-18 2016-09-29 株式会社島津製作所 Liquefied carbon dioxide supply pump and supercritical fluid chromatograph
EP3318829A1 (en) * 2016-11-04 2018-05-09 General Electric Technology GmbH System and method for producing liquid carbon dioxide
WO2019049744A1 (en) * 2017-09-06 2019-03-14 伸和コントロールズ株式会社 Fluid supply device

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018071884A1 (en) * 2016-10-14 2018-04-19 Supercritical Fluid Technologies, Inc. Cooling loop with a supercritical fluid system using compressed refrigerant fluid flow with a positive joule-thomson coefficient

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5465581A (en) * 1993-08-24 1995-11-14 Hewlett-Packard Analytical system having energy efficient pump
US20100040483A1 (en) * 2008-06-24 2010-02-18 Berger Terry A Compressible fluid pumping system
JP2010101875A (en) * 2008-09-29 2010-05-06 Jasco Corp Device and method for injecting sample in supercritical fluid chromatography
US20140190183A1 (en) * 2010-05-26 2014-07-10 Agilent Technologies, Inc. Efficient chiller for a supercritical fluid chromatography pump
US20130334117A1 (en) * 2011-03-10 2013-12-19 Waters Technologies Corporation System and method of cooling a pump head used in chromatography
JP2012220030A (en) * 2011-04-04 2012-11-12 Toyo Eng Works Ltd Defrosting device of carbon dioxide circulation and cooling system
JP2016173343A (en) * 2015-03-18 2016-09-29 株式会社島津製作所 Liquefied carbon dioxide supply pump and supercritical fluid chromatograph
CN105986993A (en) * 2015-03-18 2016-10-05 株式会社岛津制作所 Liquid carbon dioxide delivery pump, and supercritical fluid chromatograph provided with the same
EP3318829A1 (en) * 2016-11-04 2018-05-09 General Electric Technology GmbH System and method for producing liquid carbon dioxide
WO2019049744A1 (en) * 2017-09-06 2019-03-14 伸和コントロールズ株式会社 Fluid supply device

Also Published As

Publication number Publication date
JPWO2020250317A1 (en) 2020-12-17
US20220229024A1 (en) 2022-07-21
US12044662B2 (en) 2024-07-23
CN113939736B (en) 2024-06-25
JP7342946B2 (en) 2023-09-12
WO2020250317A1 (en) 2020-12-17

Similar Documents

Publication Publication Date Title
JP6432404B2 (en) Liquefied carbon dioxide pump and supercritical fluid chromatograph equipped with it
JP4569633B2 (en) Analysis method and apparatus by liquid chromatography
JP6107538B2 (en) Column oven and liquid chromatograph
US20200032780A1 (en) Liquid delivery device and fluid chromatograph
US11237137B2 (en) Convectively controlled adiabatic column chamber for use in chromatographic systems
KR20140113881A (en) Direct injection phase change temperature control system
JP6428410B2 (en) Liquefied carbon dioxide pump and supercritical fluid chromatograph equipped with it
CN113939736A (en) Liquefied carbon dioxide supply device and supercritical fluid device
GB2495777A (en) Flow sensor stabilisation by adjusting temperature gradient
EP3132258B1 (en) Passive column pre-heater for use in chromatographic systems
US20190264670A1 (en) Thermal pump for fluid near a phase transition
CN110168344A (en) Ingredient extraction equipment
JP2016008908A (en) Component extraction separation apparatus and component extraction separation method using supercritical fluid
JPWO2016088252A1 (en) Sample recovery mechanism and supercritical fluid apparatus equipped with the sample recovery mechanism
JP7294417B2 (en) MOBILE PHASE TEMPERATURE CONTROLLER FOR SUPERCRITICAL FLUID DEVICE AND SUPERCRITICAL FLUID DEVICE
KR20200129985A (en) Chiller apparatus for semiconductor process
JPWO2019176143A1 (en) Supercritical fluid separator
CN107614079B (en) Cooling of pump heads in carbon dioxide chromatography systems
EP0716302A2 (en) Liquid chromatography system and method for thermally stabilizing several columns of a liquid chromatography system

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant